Evaluation of uncertainty in determination of carbon, hydrogen and nitrogen content in coal by using elemental analyzer
GONG Wanli
针对煤中碳氢氮含量的测量不确定度进行评定, 可提高实验室检测碳氢氮含量数据的准确性以及提升实验室检测的相应技术水平。采用vario MACRO cube 型全自动元素分析仪测定煤中碳、氢、氮元素含量, 分析不确定度的来源以建立整个测定过程中不确定度分量的数学模型,并讨论测定过程中测量重复性引入的不确定度、曲线标定时试剂纯度引入的不确定度、用标准煤样确定仪器日校正因子时引入的不确定度、样品称量时引入的不确定度以及仪器示值误差引入的不确定度, 计算测定煤中碳、氢、氮含量的合成标准不确定度及扩展不确定度。煤中碳、氢、氮含量及其置信区间分别为50. 88%±0. 61%、6. 04%±0. 22%、0. 15%±0. 03%, 其中k =2。各不确定度来源中, 使用标准煤样确定仪器校正因子对测定结果的不确定度起主导作用, 应严格控制校正过程, 选择合适的标准煤样, 可有效控制不确定度在较低水平, 提高样品检验检测的准确度。
Evaluating the uncertainty of measurement of carbon, hydrogen and nitrogen content in coal could improvethe accuracy of data of carbon, hydrogen and nitrogen content determined by laboratory and improve the correspond⁃ing technical level of laboratory testing. Vario MACRO cube automatic elemental analyzer was used to determine car⁃bon, hydrogen and nitrogen content in coal. The sources of uncertainty were analyzed. The mathematical model ofthe uncertainty component were established. The uncertainty components such as repetition of determination, reagentpurity at curve calibration, determination of daily calibration factor of instrument by using standard coal samples,sample weighing and instrument indication error were discussed. The combined standard uncertainty and extended un⁃certainty of the carbon, hydrogen and nitrogen content in coal sample were calculated. The content of carbon, hydro⁃gen and nitrogen in coal sample and their confidence intervals were: 50. 88%±0. 61%, 6. 04%±0. 22%, 0. 15%±0. 03%, among which k = 2. Among these sources of uncertainty, daily calibration factor of instrument by usingstandard coal samples played a leading role in the uncertainty of the measurement results. The correction process should be strictly controlled, and the appropriate standard coal samples should be selected to effectively control theuncertainty at a low level, so that the accuracy of measurement could be improved.
element analyzer; carbon, hydrogen and nitrogen content; evaluation of uncertainty; indication error; accuracy; confidence interval; mathematical model
主办单位:煤炭科学研究总院有限公司 中国煤炭学会学术期刊工作委员会